Process of recovering glycerin.



No. 63|,396- I Patented Aug.A 22, |899` J. DE nlEsBAci-i.

PROCESS 0F RECOVERING GLYCERIN.

(Application ld May 24, 1898.)

(No Modal.)

VMM.

7%/ f 22,/,Z Y In;

. duction or Extraction 'ofGl'ycerin from Wastey Products, 'offwhieh the following'is a specifi-l Io l y v wine,

It can therefore be e Darren STATES "PATENT Ofrllcri.

JEANNE, nnnias'imoii, ory NEAR MONTDIDIER'; reason.

SPECIFICAT-IN forming` part of Ijetters Patent N o.

Roenes 0F REoo'i/ERING. cLYcE'RiN.

631,396, dated August `22, ieee.

Application tiled My 24, 1,898- SerialvNo. 681,620. (No specimens.)

vTo all. whom' it muy concern:

Be it known that I, JEANNE DE DlnsBAoH, (ne J EANNE DE BEAUREPAIRE LoUvAGNY,) residing at the Chateau de Reinaugies, near Montdidier, in the Department' ofthe in the Republic of France, have invented eertain new anduseful Improvements in the Procation. y A *The wash relating to the distillation of tion contains glycerin, which is formdd during the alcoholic fermentation at the expensev .of thes'ugar." Thisglycerin, partly drawn over by the ebu-llition, is retained by the distilling-eolumn or by the analyzing apparatus.

recovered from these residues, in which it is lost under vordinary circumstances. f

The object of this invention is to extract the glycerin from Athe wash. or residue. By the term wash is meant residues of all kinds found in reterts or alembies after the process of distilling wines, grain, molasses, beet-root, or, in other words, the residues of any alcoholic fermentation.

The process consists, essentially, invii rst evaporating the Wash to a suitable degreeiu a closed reeeptaelmso as to enable the salts to deposit, in 'subsequently neutralizing `this evaporatedwash or residue by means of a snitable chemical agent, and in finally causing superheated steam .to pass into this concentrated wash at an appropriate temperature, so as to disaggregate the mass and to carry otlf the glycerin, which is condensed in'a suitable ap` paratus provided for this purpose.

In order to carry the process into practice, thedistillers wash to lbe treat-ed is so evaporated as to reduce the sanne to a suitable degree of concentration; This concentration is preferably effected ina closed Vessel in order to enable the salts-fsueh as tart-ratos, chlorids andsulfates of potassium, iron, alumini# um, calcium, andphosphates of ealcium-to deposit. VThis deposition oi' the salts is advantageous, because by ridding the wash thereof the chances of injurious combinations occurring in the subsequent treatment are Somme,

grain, molasses,l beet-root, and,l speak-` ing generally, from any alcoholicfermentais greater.

preferably effected by o a heat not greater than decompose :the glycerin at tliedistilling-.temperatureailllt is, therefore'iniportant :to neurom its salts is treated bya suitable neutrallime, being preferably employed for the purose. The quantity of lime employed natuiallyyaries and depends upon the'quantity of free acids in the wash which it is neces'- sary to fix. The lime salts, such as sulfatos and tartrates, are precipitated and gathered with the excess of lime, il any, at the bottoni salts and lime beingadded to themass to be` subsequently distilled and the forming by-prodnets.

rlhe third operation consists in treating the 'concentrated wash after it has been freed from the greater part of its salts and after its that the glycerin may be vaporized without being, however, decomposed. For thislatter operation a separating apparatus maybe used of the kind, for example, which are at the present time employed in sten-rin vor soap works for the distillation of the raw glycerin. Finally, the condensed `glycerin collected in the condenser is purified by any suitable means, according tothe impurities'contained therein, which are dependent upon the. varying nature of the wash treated and upon the degree of purity desired to be obtained.

T he degree of concentratonof 'thefwashof 1 lime and salts,

neutralization with superheated steain,whieh must be of a suitable temperature in order far less andthe quantity of'glye'erin obtained f not combinedwith afbase to form salts would j tralize them,and in order to eiect this the con- Q; centuatedwash after it hasbe'en partly freed.

'lzing agent, lime, either in powder or milk oli of the tanks, the yliquid extracted. from`the.

In the accompanying drawing the figure illustrates, diagram matically, one form of apparatusfor carrying onttheimproved process.

As shown, the apparatus is composed of a. furnace a, a retort b, tvvo coils c and d, surrounded by a tank e, and two closed receiving vesselsfand g. The hot gases produced by combustion leave, the hearth a', and following the dire'c'ti'ouoll the arrows on account ofthebaflie-plates t? enter the flue d, running spirally around the retort b, and escape by the chimney-opening di. Vhen the temperature in the retort is sufficiently high, which can he seen by the thermometerlrdipping into it, the damper t5 is closed anlltnpened, so that the hot gases escape by the openinga.

Tubes t', containing steam to be superheated, are placed in the furnace in such a way as to give the greatest possible heatingsurface. The tubes are all united and the end one passes into the retort, where after forming a coil it finishes in a rose i, placed at tlfebottom of the retort. This rose has only holes at) he sides, which allow the super- 'heated steam to penetrate the mass contained in the retort, carrying with it the ammonia y and glycerin. The ammonia being much I more volatile than the glycerin passes by the i, upper tube c, the tap d being closed. This tube c descends to the tank e, filled with cold Water, and passing through it in a coil con- 'l ducts the ammonia into the closed vessel g. \Vhen all the ammonia is extracted, the glycerin begins to be carried along by the superl heated steam. The tap c' is then closed and 35 opened. The glycerin descends by the pipe c1, which passes in a coil through the tank filled with cold water and conducts it to the closed vessel f.

The retort is putinto communication with 4o an ejectork by means of a tube provided with a vacuum-gage 7c'. The residues or washes are contained in a vesselarr and are introduced into the retort by the funnel y, closed by a valve y'. The retort has also a blow-off cock l. The superheated steam-supply pipe has a/ pressure-gage and tap.

Having,r now particularly described and s certained the nature of my said invention and in what manner the sameis to be performed, what I claim is The process of extracting glycerin from a wash containing the same which consists in concentrating the wash by evaporation, in treating the concentrated wash with an agent to neutralize the free acids contained therein, then subjecting the wash thus treated to the action of steam to carry off the glycerin contained therein, and finally condensing the glycerin, substantially as described.

In testimony whereof I have signed my naine to this specification in the presence of two `subscribing witnesses.

JEANXE DE DIESBACII, NE JEANNE DE BEACREPIRE LOIYAGNY. Witnesses:

EDWARD I. MACLEAN, JOHN A. NILES. 

